CN114196228A - Novel caramel-color food additive and preparation method thereof - Google Patents

Novel caramel-color food additive and preparation method thereof Download PDF

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Publication number
CN114196228A
CN114196228A CN202111624975.8A CN202111624975A CN114196228A CN 114196228 A CN114196228 A CN 114196228A CN 202111624975 A CN202111624975 A CN 202111624975A CN 114196228 A CN114196228 A CN 114196228A
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food additive
caramel color
acid
novel
heating
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谢文明
魏廉
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Aipu Food Industry Co ltd
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Aipu Food Industry Co ltd
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09BORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
    • C09B61/00Dyes of natural origin prepared from natural sources, e.g. vegetable sources
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L5/00Preparation or treatment of foods or foodstuffs, in general; Food or foodstuffs obtained thereby; Materials therefor
    • A23L5/40Colouring or decolouring of foods
    • A23L5/42Addition of dyes or pigments, e.g. in combination with optical brighteners
    • A23L5/43Addition of dyes or pigments, e.g. in combination with optical brighteners using naturally occurring organic dyes or pigments, their artificial duplicates or their derivatives
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07HSUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
    • C07H1/00Processes for the preparation of sugar derivatives
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07HSUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
    • C07H15/00Compounds containing hydrocarbon or substituted hydrocarbon radicals directly attached to hetero atoms of saccharide radicals
    • C07H15/20Carbocyclic rings
    • C07H15/203Monocyclic carbocyclic rings other than cyclohexane rings; Bicyclic carbocyclic ring systems
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23VINDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
    • A23V2002/00Food compositions, function of food ingredients or processes for food or foodstuffs

Abstract

The invention discloses a novel caramel color food additive and a preparation method thereof, and the preparation method comprises the following steps: adjusting the pH of the sucrose solution to 2-4 with acid; heating for dehydration reaction; reacting polyphenol compounds with dehydrated cane sugar under the heating condition; heating the system to 140-150 ℃ and carrying out vacuum dehydration; finally, hot water and alkali are added for modulation, and the required caramel color is obtained. The caramel color system prepared by the invention has relatively higher molecular weight, can achieve better coloring effect under the condition of adding smaller amount, and also has better oxidation resistance.

Description

Novel caramel-color food additive and preparation method thereof
Technical Field
The invention relates to the field of food additives, in particular to a novel caramel-color food additive and a preparation method thereof.
Background
Caramel, commonly known as caramel, is a substance that is coked when sugar is heated to above 130 deg.C, is a viscous liquid or powder made from maltose, sucrose, etc., is dark brown, has bitter taste, and is mainly used for coloring soy sauce, candy, vinegar, beer, etc. Caramel is an edible colorant with wide application range in food and is an important member in food additives.
With the development of the food industry, caramel color is applied more and more, and simultaneously, more requirements are put on caramel color, such as the requirement of acid resistance is put on caramel color in coca cola, and the requirement of low bitter taste is put on caramel in dessert industry.
The above needs are gradually solved in the technical progress, the market puts higher demands on oxidation resistance, and the current means is mainly to add a certain amount of antioxidant in the caramel color, but the antioxidant brings some problems. Several years ago, experts have questioned the addition of antioxidants to their diets and even have studied that these substances are involved in the development of some cancers such as prostate cancer. Therefore, there is a strong need to improve the oxidation resistance of caramel by improving its color.
Disclosure of Invention
In order to solve the problems, the invention provides a novel caramel-color food additive with good anti-oxidation performance and a preparation method thereof.
The technical scheme of the invention is as follows:
a preparation method of a novel caramel color food additive comprises the following steps:
(1) adding a certain amount of acid into the sucrose solution to adjust the pH to 2-4;
(2) then heating the sucrose solution to 100-120 ℃ for dehydration reaction until the system quality is stable;
(3) adding polyphenol compound into the system, heating the system to 130-140 ℃, and reacting for 2-4 hours;
(4) then heating the system to 140 ℃ and 150 ℃, and simultaneously carrying out vacuum dehydration for 2-4 hours;
(5) stopping the reaction, adding water and alkali at the temperature of 60-90 ℃ to obtain the required caramel color after modulation.
Further, the sucrose solution in the step (1) is an aqueous solution with 60-80% of sucrose solid content. Specifically, since the pH of the sucrose solution needs to be adjusted by acid, the solid content of the sucrose solution affects the addition amount of the acid and the viscosity of the overall reaction, and a reasonable solid content range is finally determined after considering various factors.
Further, in the step (1), the acid is one or more of sulfuric acid and phosphoric acid.
Further, the polyphenol compound in the step (3) is selected from one or more of caffeic acid, chlorogenic acid, gallic acid and protocatechuic acid.
Specifically, the invention utilizes the dehydration reaction of phenolic hydroxyl which shows weak acidity on the structure of the polyphenol compound and hydroxyl on sucrose molecules to form a-C-O-C-crosslinking structure, and the reaction principle is as follows:
Figure BDA0003438565100000021
the above reaction principle is only used to illustrate the process of the present invention, R1And R2The position and number of the units are not particularly limited, and may be changed according to the actual situation.
Further, the vacuum condition in the step (4) is 600-. Specifically, the vacuum condition should be slowly reduced from 1000mbar to achieve the purpose of removing moisture, so that the reaction of the polyphenol structure and the hydroxyl structure can be carried out forward.
Further, the temperature of the water in the step (5) is preferably 60 to 80 ℃.
Further, the alkali in the step (5) is sodium hydroxide, and a sodium hydroxide solution with a mass concentration of 10-50% is preferably prepared when the alkali is used.
The invention also provides a novel caramel color food additive prepared by the preparation method, and the molecular weight of the novel caramel color food additive is 15-20 ten thousand.
The technical scheme provided by the invention has the beneficial effects that:
according to the invention, the polyphenol-based structure is used for crosslinking with sucrose molecules, so that the molecular weight of the whole caramel color polymer can be remarkably improved, and the coloring capability of the caramel color polymer is obviously higher than that of a commercial product, so that the expected coloring effect can be achieved under the condition of adding a smaller amount of caramel color.
Compared with the unsaturated ester structure of the-C-O-CO-obtained by the traditional method, the cross-linked structure of the-C-O-C-has better stability and is less prone to oxidation. In addition, the caramel color is more acid-resistant and alkali-resistant than the traditional structure in the preparation process, so that the alkaline hydrolysis condition can not occur in the hot alkaline solution treatment process, and the whole process is more stable and controllable. The caramel color prepared by the invention has very good oxidation resistance and has wide application space in the future.
Detailed description of the invention
The present invention will be further described below by way of specific examples.
In the following examples, those whose operations are not subject to the conditions indicated, are carried out according to the conventional conditions or conditions recommended by the manufacturer.
Example 1
A novel caramel-colored food additive is prepared by the following preparation method:
(1) adding a certain amount of sulfuric acid into 1000g of a 70% solid content sucrose aqueous solution to adjust the pH to 3;
(2) then heating the sucrose solution to 110 ℃ for reaction, and carrying out dehydration reaction until the system quality is stable and unchanged;
(3) 10g of polyphenol compound caffeic acid (structural formula is shown in the specification)
Figure BDA0003438565100000031
) Adding the mixture into a system, and heating the system to 130 ℃ for reaction for 3 hours;
(4) then heating the system to 145 ℃, controlling the vacuum degree to carry out vacuum dehydration under 600mbar, and reacting for 3 hours;
(5) reducing the temperature of the system to 60-80 ℃ after the reaction is finished, and adding hot water of 80 ℃ and sodium hydroxide solution with the concentration of 30% for modulation to obtain the required caramel color food additive.
Example 2
A novel caramel-colored food additive is prepared by the following preparation method:
(1) adding a certain amount of sulfuric acid into 1000g of a sucrose aqueous solution with the solid content of 80% to adjust the pH to 2.5;
(2) then heating the sucrose solution to 100 ℃ for reaction, and carrying out dehydration reaction until the system quality is stable and unchanged;
(3) 10g of polyphenol compound chlorogenic acid (structural formula is shown in the specification)
Figure BDA0003438565100000041
) Adding the mixture into a system, and heating the system to 130 ℃ for reaction for 3 hours;
(4) then heating the system to 145 ℃, controlling the vacuum degree to carry out vacuum dehydration under 700mbar, and reacting for 2 hours;
(5) reducing the temperature of the system to 60-80 ℃ after the reaction is finished, and adding hot water of 80 ℃ and sodium hydroxide solution with the concentration of 30% for modulation to obtain the required caramel color food additive.
Example 3
A novel caramel-colored food additive is prepared by the following preparation method:
(1) adding a certain amount of sulfuric acid into 1000g of 60% solid content sucrose aqueous solution to adjust the pH to 3;
(2) then heating the sucrose solution to 120 ℃ for reaction, and carrying out dehydration reaction until the system quality is stable and unchanged;
(3) 10g of polyphenol compound gallic acid (structural formula is shown in the specification)
Figure BDA0003438565100000042
) Adding the mixture into a system, and heating the system to 130 ℃ for reaction for 3 hours;
(4) then heating the system to 145 ℃, controlling the vacuum degree to carry out vacuum dehydration under 700mbar, and reacting for 3 hours;
(5) reducing the temperature of the system to 60-80 ℃ after the reaction is finished, and adding hot water of 80 ℃ and sodium hydroxide solution with the concentration of 30% for modulation to obtain the required caramel color food additive.
Example 4
A novel caramel-colored food additive is prepared by the following preparation method:
(1) adding a certain amount of sulfuric acid into 1000g of a 70% solid content sucrose aqueous solution to adjust the pH to 3.5;
(2) then heating the sucrose solution to 110 ℃ for reaction, and carrying out dehydration reaction until the system quality is stable and unchanged;
(3) 10g of protocatechuic acid (structural formula
Figure BDA0003438565100000051
) Adding the mixture into a system, and heating the system to 130 ℃ for reaction for 3 hours;
(4) then heating the system to 145 ℃, controlling the vacuum degree to carry out vacuum dehydration under 700mbar, and reacting for 3 hours;
(5) reducing the temperature of the system to 60-80 ℃ after the reaction is finished, and adding hot water at 80 ℃ and a sodium hydroxide solution with the concentration of 30% for modulation to obtain the required caramel color food additive.
Example 5
A novel caramel-colored food additive is prepared by the following preparation method:
(1) adding a certain amount of sulfuric acid into 1000g of a 70% solid content sucrose aqueous solution to adjust the pH to 3;
(2) then heating the sucrose solution to 110 ℃ for reaction, and carrying out dehydration reaction until the system quality is stable and unchanged;
(3) adding 20g of polyphenol compound caffeic acid into the system, and heating the system to 130 ℃ for reaction for 3 hours;
(4) then heating the system to 145 ℃, controlling the vacuum degree to carry out vacuum dehydration under 600mbar, and reacting for 4 hours;
(5) reducing the temperature of the system to 60-80 ℃ after the reaction is finished, and adding hot water of 80 ℃ and sodium hydroxide solution with the concentration of 30% for modulation to obtain the required caramel color food additive.
Example 6
A novel caramel-colored food additive is prepared by the following preparation method:
(1) adding a certain amount of sulfuric acid into 1000g of a 70% solid content sucrose aqueous solution to adjust the pH to 3;
(2) then heating the sucrose solution to 110 ℃ for reaction, and carrying out dehydration reaction until the system quality is stable and unchanged;
(3) adding 20g of polyphenol compound gallic acid into the system, and heating the system to 130 ℃ for reaction for 3 hours;
(4) then heating the system to 145 ℃, controlling the vacuum degree to carry out vacuum dehydration under 600mbar, and reacting for 4 hours;
(5) reducing the temperature of the system to 60-80 ℃ after the reaction is finished, and adding hot water of 80 ℃ and sodium hydroxide solution with the concentration of 30% for modulation to obtain the required caramel color food additive.
Example 7
A novel caramel-colored food additive is prepared by the following preparation method:
(1) adding a certain amount of sulfuric acid into 1000g of a 70% solid content sucrose aqueous solution to adjust the pH to 3;
(2) then heating the sucrose solution to 110 ℃ for reaction, and carrying out dehydration reaction until the system quality is stable and unchanged;
(3) adding 20g of polyphenol compound chlorogenic acid into the system, and heating the system to 130 ℃ for reaction for 3 hours;
(4) then heating the system to 145 ℃, controlling the vacuum degree to carry out vacuum dehydration under 600mbar, and reacting for 4 hours;
(5) reducing the temperature of the system to 60-80 ℃ after the reaction is finished, and adding hot water of 80 ℃ and sodium hydroxide solution with the concentration of 30% for modulation to obtain the required caramel color food additive.
And (3) performance testing:
the molecular weight, absorbance and oxidation resistance of the products prepared in examples 1 to 7 and the commercial products were measured, respectively, and the results are shown in table 1, and the test methods are as follows:
average molecular weight test: the test was carried out using the aqueous phase GPC method.
And (3) absorbance test: the tests were carried out according to the method of GB 1886.64-2015. Weighing 0.5g of sample, accurately measuring to 0.002g, dissolving with water, transferring to a 500mL volumetric flask, adding water to dilute to a scale, shaking up, and centrifugally settling if the solution is turbid to obtain a sample solution. The sample solution was placed in a 1cm cuvette, and the absorbance at 610nm was measured with a spectrophotometer using water as a blank.
Oxidation resistance test (test DPPH radical scavenging capacity): preparing 1.5mL of 0.5mg/mL caramel solution, adding 1.5mL of 0.1mmol/L DPPH ethanol solution, mixing well, and standing at room temperatureReacting for 30min in the dark, and testing the light absorption value A at the wavelength of 517nm1(ii) a 1.5mL of ethanol solution replacing DPPH and 1.5mL of 0.5mg/mL caramel solution are mixed uniformly, then the mixture is reacted for 30min in a dark place at room temperature, and the light absorption value A is measured at the wavelength of 517nm2(ii) a 1.5mL of deionized water instead of the sample solution and DPPH ethanol solution are reacted for 30min in a dark place, and the light absorption value A is measured at the wavelength of 517nm0
DPPH radical clearance (%) {1- (a)1-A2)/A0)}*100
The absorbance characterizes its coloring power, the greater the absorption intensity, the stronger its coloring power.
TABLE 1
Figure BDA0003438565100000071
As can be seen from the above Table 1, the caramel color prepared by the invention has relatively larger molecular weight, and can achieve better coloring effect under the condition of adding smaller amount; in addition, the caramel color prepared by the invention has better antioxidant effect and high stability.
The above-mentioned serial numbers of the embodiments of the present invention are merely for description and do not represent the merits of the embodiments.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.

Claims (9)

1. A preparation method of a novel caramel color food additive is characterized by comprising the following steps:
(1) adding a certain amount of acid into the sucrose solution to adjust the pH to 2-4;
(2) then heating the sucrose solution to 100-120 ℃ for dehydration reaction until the system quality is stable;
(3) adding polyphenol compound into the system, heating the system to 130-140 ℃, and reacting for 2-4 hours;
(4) then heating the system to 140 ℃ and 150 ℃, and simultaneously carrying out vacuum dehydration for 2-4 hours;
(5) stopping reaction, adding hot water at 60-90 deg.C and alkali, and concocting to obtain the desired caramel color.
2. The method for preparing a novel caramel color food additive as claimed in claim 1, wherein the sucrose solution in step (1) is an aqueous solution with 60-80% sucrose solid content.
3. The method for preparing a novel caramel color food additive as claimed in claim 1, wherein the acid in step (1) is one or more of sulfuric acid and phosphoric acid.
4. The method for preparing a novel caramel color food additive according to claim 1, wherein the polyphenol compound in the step (3) is selected from one or more of caffeic acid, chlorogenic acid, gallic acid and protocatechuic acid.
5. The method for preparing the caramel color food additive as claimed in claim 1, wherein the vacuum condition in step (4) is 600-800 mbar.
6. The method for preparing a novel caramel color food additive as claimed in claim 1, wherein the temperature of the water in step (5) is 60-80 ℃.
7. The method for preparing a novel caramel color food additive as claimed in claim 1, wherein the alkali in step (5) is sodium hydroxide.
8. A novel caramel-colored food additive produced by the production process according to any one of claims 1 to 7.
9. The novel caramel color food additive as claimed in claim 8, wherein the molecular weight of the caramel color food additive is 15 to 20 ten thousand.
CN202111624975.8A 2021-12-28 2021-12-28 Novel caramel-color food additive and preparation method thereof Pending CN114196228A (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113136113A (en) * 2021-04-23 2021-07-20 上海爱普食品工业有限公司 Method for improving oxidation resistance of caramel color by gradient reaction
CN113209913A (en) * 2021-04-26 2021-08-06 上海爱普食品工业有限公司 Preparation method of caramel-colored hydrogel

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113136113A (en) * 2021-04-23 2021-07-20 上海爱普食品工业有限公司 Method for improving oxidation resistance of caramel color by gradient reaction
CN113209913A (en) * 2021-04-26 2021-08-06 上海爱普食品工业有限公司 Preparation method of caramel-colored hydrogel

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
谭榀新等: "植物提取物抗氧化成分及机理研究进展", 食品科学, vol. 31, no. 15, pages 288 - 292 *

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